Nickel salt and process of making same.



FFICE.

HANS A. FRASOH, OF HAMILTON, CANADA.

SPECIFICATION forming" part of Letters Patent No. 669,899, dated March12, 1901.

Application filed November 7, 1900.

T0 aZZ whom it may concern.-

Be it known that I, HANS A. FRASCH, a citizen of the United States,residing at Hamilton, in the county of Wentworth and Province ofOntario, Canada, have invented a certain new and useful Nickel Salt andProcess of Making Same, of which the following is a full, clear, andexact description.

The object of thisiuvention is the production of a nickel salt which maybe employed directly for nickel-plating and for other purposes.

The invention consists of the nickel salt having the characteristics andproperties hereinafter specified and in the method of separating suchsalt from a solution containing nickel alone or combined with othermetallic salts.

I find that a salt of nickel and ammonium in certain proportions isnearly insoluble in a concentrated salt solution and that thenickel-ammonium salt, while readily soluble in water, can beprecipitated from an aqueous solution by the addition of another solublesalt, such as sodium chlorid or potassium chlorid or sulfate or anyother soluble salt which Will not combine with or contaminate thenickel-ammonium salt.

In carrying out my invention I absorb ammonia-gas in a solution of anickel salt, such asthe sulfate or chlorid, until all the nickel andother metals in the solution which are capable of combining with ammoniaare transformed into the corresponding ammonium salt, leaving a slightexcess of ammonia, or a mixture of metallic salts containing nickel maybe exposed in a dry state to the action of ammonia or ammonium carbonateuntil the salts are converted into the ammonium salts, and these lastmay then be dissolved in Water, and to this solution of metallicammonium salts is added sodium chlorid until at a certain saturation ofthe solution with sodium chlorid a nickel-ammonium salt containingapproximately six equivalents of ammonia to every one of nickel isprecipitated, the addition of sodium chlorid being continued untilprecipitation ceases. Of these six equivalents of ammonia two are inchemical combination with the nickel and chlorin and four exist as freeammonia. Instead of sodium chlorid I may use potassium chlorid ammoniumsalt.

Serial No. 35,744. (No specimens.)

or any other salt which will displace the nickel- Furthermore, insteadof treating the metallic salts or a solution thereof with am mouia-gasammoniacal solution may be used, in which case the metallicsalt solutionmay be saturated with sodium chlorid or other suit-able salt, to whichis added a solution of am monia of 26 Ban me in strength, which lattersolution may be previously saturated with sodium chloride or other saltin sufficient quantity to precipitate the nickel salt.

In carrying out my invention with a solution consisting of the chloridsof several metals as, forinstance, the chlorids of iron, copper, cobalt,and nickelI first remove the iron by precipitation with calciumcarbonate after previous oxidation, if necessary, and separate theprecipitate by filtration or other suitable means. I then saturate thesolution with ammonia or add to it aconcentrated solution of ammonia ofabout 26 Baume in strength until the metallic salts are con verted intoammonium salts,after which is added sodium chlorid or a solutionthereof, upon which a nickel-ammonium salt separates in the form of acrystalline precipitate of purple or violet color. The addition ofsodium chlorid is continued until no more precipitate is formed, andwhen this point is reached no more than two one-hundredths of one percent. (0.02) of nickel remains in the solution. The precipitatednickel-ammonium salt is separated by filtration and washed with asaturated solution of sodium chlorid containing free ammonia and is thendried in any ordinary manner. The ammonia contained in the residualfiltrate may be recovered by distillation, and the copper and cobalt maybe removed chemically or by other means.

My salt may be produced from the normal nickel-ammonium chlorid orsulfate by additain: nickel, 24.7; chlorin,30.6; ammonium, (combined asNH 14.7; ammonia, (free or combined,) 26.5; cobalt, (as an impurity,)0.05; sodium chlorid, (as an impurity,) 1.81;

moisture, (as an impurity,) 1.6; total, 99.96. This nickel-ammoniumsalton present determination corresponds to the chemical formula Ni-(NHOl +4NH The salt is of purple (violet) color, crystalline, veryhygroscopic, and if precipitated from a concentrated salt solution itforms a fine powder of minute crystals, while if dissolved to saturationin hot water large crystals are formed upon cooling which are quadraticin form and of dark-blue or sapphire color. If ex posed to dry air, partof its ammonia evaporates and the color changes from purple to green.Exposed to moist air it absorbs the moisture and liquefies, forming adark-green solution. iug a blue solution, and parts with some ofits ammonia. If exposed to atmospheric air or if part of its ammonia has beenallowed to evaporate, it forms a turbid solution which becomes clearupon the addition of ammonia. If boiled in aqueous solution, two-thirdsof the ammonia contents evaporate and a green precipitate is formed. Thedry salt smells slightly of ammonia and if moistened or dissolveddevelops a strong odor of ammonia.

It differs from the normal nickel-ammonium chlorid or sulfate in thegreat excess of ammonia it contains, there being about six equivalentsof am monia to every one of nickel,

two of saidequivalents of ammonia beingin chemical combination with thenickel and chlorin and four existing as free ammonia.

l/Vhat I claim is l. The herein-described nickel salt, consisting of adouble salt of nickel-ammonium chlorid and four equivalents of freeammonia.

2. The herein-described nickel salt, consisting of nickel, chlorin, andammonia, and possessing the constitution represented by the formula:

3. A nickel salt possessing the constitution represented by the formula:

forming a crystalline mass of violet color, very hygroscopic, freelysoluble in water,with

It is readily soluble in Water,l''orma blue color and emitting a strongodor of ammonia.

4. The process of producing a nickel salt, consisting in combiningammonia in excess with a salt of nickel, and precipitating suchammonium-nickel salt from a solution by means of a salt capable ofdisplacing the same.

5. The process of separating a nickel-ammonium salt from a solution,consisting in precipitating the nickel-ammonium salt by dissolving inthe solution a salt capable of displacing the nickel-ammonium salt fromits solution.

6. The process of prod ucing an ammoniumnickel salt, which consists in.saturating a solution containing nickel salt with ammonia until anexcess of ammonia is present, and precipitating from the solution thenickelammonium salt by the addition of a salt capable of displacing thenickel-ammonium salt.

7. The process of producing an ammoniuinnickel salt, which consists inabsorbing ammonia in a solution containing nickel, and displacing thenickel-ammonium salt thereby obtained by the addition of sodium chlorid.

8. The process of separating nickel from copper and cobalt and othermetals Whose hydroxids are soluble in ammonia, consisting in absorbingin a solution of the salts of those metals ammonia in excess, and addingto the solution of metallic ammonium salts thereby obtained a saltcapable' of displacing the nickel-ammonium salt.

9. The process of separating nickel from a metallic salt containing thesame, consisting in absorbing ammonia in excess in a solution of thesalt, adding to the solution a salt capable of displacing thenickel-ammonium salt until precipitation ceases, filtering out thenickel-ammonium salt, washing the filtrate with a saturated solution ofsodium chlorid containing free ammonia, and then drying.

In testimony whereof I have hereunto set 5 my hand this 5th day ofNovember, A. D. 1900.

HANS A. FRASCH.

Witnesses:

ANNA M. HERRIMAN, GEO. T. SELLENs.

